CN112599745B - Porous NiCo2O4Positive electrode material coated with lithium nickel cobalt aluminate and preparation method thereof - Google Patents
Porous NiCo2O4Positive electrode material coated with lithium nickel cobalt aluminate and preparation method thereof Download PDFInfo
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- PFYQFCKUASLJLL-UHFFFAOYSA-N [Co].[Ni].[Li] Chemical compound [Co].[Ni].[Li] PFYQFCKUASLJLL-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims description 7
- 239000007772 electrode material Substances 0.000 title description 2
- 239000002135 nanosheet Substances 0.000 claims abstract description 57
- 238000010438 heat treatment Methods 0.000 claims abstract description 53
- 229910005949 NiCo2O4 Inorganic materials 0.000 claims abstract description 35
- 229910002995 LiNi0.8Co0.15Al0.05O2 Inorganic materials 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000004202 carbamide Substances 0.000 claims abstract description 25
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 20
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000010405 anode material Substances 0.000 claims abstract description 17
- 229910018632 Al0.05O2 Inorganic materials 0.000 claims abstract description 14
- 229910013716 LiNi Inorganic materials 0.000 claims abstract description 13
- 239000007774 positive electrode material Substances 0.000 claims abstract description 13
- 229910003266 NiCo Inorganic materials 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 6
- 230000007062 hydrolysis Effects 0.000 claims abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 5
- 230000009286 beneficial effect Effects 0.000 claims abstract description 4
- 238000009792 diffusion process Methods 0.000 claims abstract description 4
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims abstract description 3
- 230000005540 biological transmission Effects 0.000 claims abstract description 3
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 3
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910001429 cobalt ion Inorganic materials 0.000 claims abstract description 3
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 3
- 229910001453 nickel ion Inorganic materials 0.000 claims abstract description 3
- 230000010287 polarization Effects 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 54
- 239000002904 solvent Substances 0.000 claims description 52
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 36
- 239000012153 distilled water Substances 0.000 claims description 28
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 26
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 20
- UUCGKVQSSPTLOY-UHFFFAOYSA-J cobalt(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Co+2].[Ni+2] UUCGKVQSSPTLOY-UHFFFAOYSA-J 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 20
- 238000004080 punching Methods 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 16
- 238000004321 preservation Methods 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 12
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 12
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 10
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 10
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 10
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 8
- 239000002033 PVDF binder Substances 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 8
- 239000011888 foil Substances 0.000 claims description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 8
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 2
- 230000002238 attenuated effect Effects 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 238000013508 migration Methods 0.000 claims description 2
- 230000005012 migration Effects 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052744 lithium Inorganic materials 0.000 abstract description 6
- 238000009830 intercalation Methods 0.000 abstract 1
- 230000002687 intercalation Effects 0.000 abstract 1
- 238000005406 washing Methods 0.000 description 12
- 238000001914 filtration Methods 0.000 description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920000858 Cyclodextrin Polymers 0.000 description 1
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 239000001116 FEMA 4028 Substances 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- LMFMZUUUIFGRHQ-UHFFFAOYSA-K S(=O)(=O)([O-])F.[Fe+2].[Li+].S(=O)(=O)([O-])F.S(=O)(=O)([O-])F Chemical compound S(=O)(=O)([O-])F.[Fe+2].[Li+].S(=O)(=O)([O-])F.S(=O)(=O)([O-])F LMFMZUUUIFGRHQ-UHFFFAOYSA-K 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 description 1
- 229960004853 betadex Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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Abstract
The invention relates to the technical field of lithium ion batteries and discloses a porous NiCo2O4Nickel-cobalt lithium aluminate coated positive electrode material and LiNi with two-dimensional layered morphology0.8Co0.15Al0.05O2The nano-sheet has an ultra-high specific surface area, sites for electrochemical lithium removal and lithium intercalation are rich, hydrolysis of urea releases hydroxyl and carbonate, the hydroxyl and the carbonate interact with cobalt ions and nickel ions to form a nano needle-shaped structure, the nano needle self-assembles to form a nano sea urchin-shaped structure through an Oswald curing process to form a nano sea urchin-shaped double-metal carbonate hydroxide precursor, and NiCo is generated through high-temperature heat treatment2O4In the process, carbon dioxide and water vapor are released to form a hollow and mesoporous structure, and the porous NiCo is obtained2O4Coated LiNi0.8Co0.15Al0.05O2Lamellar nanosheets, NiCo2O4The coating effect is beneficial to reducing LiNi0.8Co0.15Al0.05O2The capacity attenuation of the anode material improves the rate capability of the anode material, promotes the diffusion and transmission of electrons and lithium ions, and reduces the polarization effect of the electrode.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to porous NiCo2O4A positive pole material coated with nickel cobalt lithium aluminate and a preparation method thereof.
Background
The lithium ion battery is a green rechargeable battery with wide application, mainly works by moving lithium ions between a positive electrode and a negative electrode, has the advantages of high energy density, high average output voltage, wide working temperature range, no memory effect, stable cycle performance, quick charge and discharge and the like, and has important application in the fields of portable electronic products and electric automobiles.
The prior lithium ion battery anode material mainly comprises transition metal oxides such as lithium cobaltate, lithium manganate, lithium nickel cobalt aluminate and the like; polyanionic compounds such as lithium iron fluorosulfate, lithium iron phosphate, and the like; wherein the nickel cobalt lithium aluminate LiNi0.8Co0.15Al0.05O2Has higher specific capacity, is a lithium ion battery anode material with great development potential, thereby further promoting LiNi0.8Co0.15Al0.05O2The actual specific capacity and rate capability of the anode material reduce the capacity attenuation thereof so as to meet the requirement of industrial development.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a porous NiCo2O4Lithium nickel cobalt aluminate-coated positive electrode material and preparation method thereof, LiNi0.8Co0.15Al0.05O2Has excellent actual specific capacity and rate capability.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: porous NiCo2O4The porous NiCo is coated with the positive electrode material of nickel-cobalt lithium aluminate2O4The preparation method of the positive electrode material coated with the nickel-cobalt lithium aluminate comprises the following steps:
(1) adding a distilled water solvent, nickel chloride, cobalt chloride and urea into a reaction bottle, stirring and dissolving, adding an ethylene glycol solvent, placing the mixture into a microwave reaction device, heating to 180 ℃ and 200 ℃, reacting for 20-40min, filtering to remove the solvent, washing with distilled water and ethanol, and drying to obtain the nickel-cobalt hydroxide nanosheet.
(2) Adding ethanol solvent, aluminum chloride and nickel cobalt hydroxide nanosheets into a reaction bottle, uniformly stirring, adding lithium hydroxide, uniformly stirring for 1-2h, heating to 120 ℃ for 100-0.8Co0.15Al0.05O2A layered nanosheet.
(3) Adding distilled water solvent and LiNi into a reaction bottle0.8Co0.15Al0.05O2Adding urea after ultrasonic dispersion of the layered nano sheets, cobalt nitrate and nickel nitrate is uniform, stirring for 1-2h, transferring the solution into a hydrothermal reaction kettle, heating to 110-2O4Coated LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(4) Adding porous NiCo to N-methylpyrrolidone solvent2O4Coated LiNi0.8Co0.15Al0.05O2Uniformly stirring the layered nanosheets, the conductive carbon black and the polyvinylidene fluoride in a mass ratio of 8:1:1 to form slurry, coating the slurry on the surface of an aluminum foil, drying, cutting by a sheet punching machine, and punching by a sheet pressing machine to obtain the porous NiCo2O4The lithium ion battery anode material coated with nickel cobalt lithium aluminate.
Preferably, the mass ratio of the nickel chloride, the cobalt chloride and the urea in the step (1) is 530-535:100: 7200-7800.
Preferably, the microwave reaction device in the step (1) comprises a microwave emitter, a motor is fixedly connected to the inner lower portion of the microwave reaction device, a rotating rod is movably connected to the motor, a rotating guide wheel is fixedly connected to the upper portion of the rotating rod, a rotating wheel tooth is movably connected to the rotating guide wheel, a loading disc is fixedly connected to the rotating wheel tooth, and a reaction bottle is arranged above the loading disc.
Preferably, the mass ratio of the aluminum chloride to the nickel-cobalt hydroxide nanosheets to the lithium hydroxide in the step (2) is 10:82-85: 23-26.
Preferably, LiNi in the step (3)0.8Co0.15Al0.05O2The mass ratio of the lamellar nano-sheets to the cobalt nitrate to the nickel nitrate to the urea is 100:2-3.2:0.6-1: 20-30.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the porous NiCo2O4The nickel cobalt lithium aluminate-coated positive electrode material is prepared by microwave reaction by respectively using cobalt chloride and nickel chloride as a cobalt source and a nickel source, under the action of hydroxyl generated by urea hydrolysis, preparing a nano flaky nickel cobalt hydroxide precursor, and further reacting with aluminum chloride and lithium hydroxide to obtain LiNi with a two-dimensional layered appearance0.8Co0.15Al0.05O2The nano-sheet structure has an ultra-high specific surface area, and sites for electrochemical lithium removal and lithium insertion are abundant.
The porous NiCo2O4In the high-temperature hydrothermal process of the nickel-cobalt lithium aluminate-coated positive electrode material, hydrolysis of urea releases hydroxyl and carbonate, the hydroxyl and the carbonate interact with cobalt ions and nickel ions to form a nano needle-shaped structure, the nano needle is self-assembled to form a nano sea urchin-shaped structure through an Oswald curing process to form a nano sea urchin-shaped double-metal carbonate hydroxide precursor, and further high-temperature heat treatment is carried out to generate NiCo2O4In the process, the precursor releases carbon dioxide and water vapor to form a hollow and mesoporous structure, thereby forming the sea urchin-shaped porous hollow NiCo2O4Coated LiNi0.8Co0.15Al0.05O2Lamellar nanosheets, NiCo2O4The coating effect is beneficial to reducing LiNi0.8Co0.15Al0.05O2The capacity of the anode material is attenuated, the rate capability of the anode material is improved, and simultaneously NiCo2O4Has good electronic conductivity and ion diffusion coefficient, and the unique sea urchin-shaped porous hollow structure can promote the migration of electrons, shorten the transmission path of lithium ions and accelerate the diffusion of the lithium ions, thereby reducing the polarization of the electrode and leading the porous NiCo2O4The positive electrode material coated with the nickel-cobalt lithium aluminate has excellent actual specific capacity and rate capability.
Drawings
FIG. 1 is a schematic front view of a microwave reaction apparatus;
figure 2 is a top view of the carrier tray.
1-microwave reaction device; 2-a microwave emitter; 3, a motor; 4-rotating the rod; 5-rotating the guide wheel; 6-rotating gear teeth; 7-carrying plate; 8-reaction flask.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: porous NiCo2O4The preparation method of the positive electrode material coated with the nickel-cobalt lithium aluminate comprises the following steps:
(1) adding a distilled water solvent into a reaction bottle, adding nickel chloride, cobalt chloride and urea with the mass ratio of 530-.
(2) Adding ethanol solvent, aluminum chloride and nickel cobalt hydroxide nanosheets into a reaction bottle, uniformly stirring, adding lithium hydroxide according to the mass ratio of 10:82-85:23-26, uniformly stirring for 1-2h, heating to 100-fold organic silicon, standing for 10-15h, placing a solid mixed product into a muffle furnace, heating to 480-fold organic silicon 520 ℃, carrying out heat treatment for 4-6h, heating to 720-fold organic silicon 760 ℃, and carrying out heat preservation and calcination for 8-12h to obtain LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(3) Adding distilled water solvent and LiNi into a reaction bottle0.8Co0.15Al0.05O2Uniformly dispersing the layered nano sheets, cobalt nitrate and nickel nitrate by ultrasonic, adding urea into the mixture at a mass ratio of 100:2-3.2:0.6-1:20-30, stirring for 1-2h, transferring the solution into a hydrothermal reaction kettle, heating to 110-130 ℃, reacting for 5-8h, filtering to remove the solvent, washing and drying by using distilled water and ethanol, placing the solid mixed product into a muffle furnace, heating to 420-480 ℃, and performing heat preservation treatment for 2-3h to obtain the poly-beta-cyclodextrin clathrate compoundPorous NiCo2O4Coated LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(4) Adding porous NiCo to N-methylpyrrolidone solvent2O4Coated LiNi0.8Co0.15Al0.05O2Uniformly stirring the layered nanosheets, the conductive carbon black and the polyvinylidene fluoride in a mass ratio of 8:1:1 to form slurry, coating the slurry on the surface of an aluminum foil, drying, cutting by a sheet punching machine, and punching by a sheet pressing machine to obtain the porous NiCo2O4The lithium ion battery anode material coated with nickel cobalt lithium aluminate.
Example 1
(1) Adding distilled water solvent, nickel chloride, cobalt chloride and urea with the mass ratio of 530:100:7200 into a reaction bottle, stirring and dissolving, adding ethylene glycol solvent, placing into a microwave reaction device, wherein the microwave reaction device comprises a microwave emitter, a motor is fixedly connected to the lower part of the interior of the microwave reaction device, the motor is movably connected with a rotating rod, a rotating guide wheel is fixedly connected to the upper part of the rotating rod, the rotating guide wheel is movably connected with a rotating gear, a carrying disc is fixedly connected with the rotating gear, a reaction bottle is arranged above the carrying disc, heating is carried out to 180 ℃, reacting for 20min, filtering and removing the solvent, washing and drying by using distilled water and ethanol to prepare the nickel cobalt hydroxide nanosheet.
(2) Adding ethanol solvent, aluminum chloride and nickel cobalt hydroxide nanosheets into a reaction bottle, uniformly stirring, adding lithium hydroxide according to the mass ratio of 10:82:23, uniformly stirring for 1h, heating to 100 ℃, standing for 10h, placing a solid mixed product into a muffle furnace, heating to 480 ℃, carrying out heat treatment for 4h, then heating to 720 ℃, carrying out heat preservation and calcination for 8h, and preparing to obtain LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(3) Adding distilled water solvent and LiNi into a reaction bottle0.8Co0.15Al0.05O2Uniformly dispersing the layered nano sheets, cobalt nitrate and nickel nitrate by ultrasonic, adding urea with the mass ratio of 100:2:0.6:20, stirring for 1h, transferring the solution into a hydrothermal reaction kettle, heating to 110 ℃, reacting for 5h, filteringRemoving the solvent, washing and drying by using distilled water and ethanol, putting the solid mixed product into a muffle furnace, heating to 420 ℃, and carrying out heat preservation treatment for 2 hours to prepare the porous NiCo2O4Coated LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(4) Adding porous NiCo to N-methylpyrrolidone solvent2O4Coated LiNi0.8Co0.15Al0.05O2Uniformly stirring the layered nanosheets, the conductive carbon black and the polyvinylidene fluoride in a mass ratio of 8:1:1 to form slurry, coating the slurry on the surface of an aluminum foil, drying, cutting by a sheet punching machine, and punching by a sheet pressing machine to obtain the porous NiCo2O4A lithium ion battery positive electrode material 1 coated with nickel cobalt lithium aluminate.
Example 2
(1) Adding distilled water solvent, nickel chloride, cobalt chloride and urea with the mass ratio of 531:100:7400 into a reaction bottle, stirring and dissolving, adding ethylene glycol solvent, placing into a microwave reaction device, wherein the microwave reaction device comprises a microwave emitter, a motor is fixedly connected to the lower part of the interior of the microwave reaction device, the motor is movably connected with a rotating rod, a rotating guide wheel is fixedly connected to the upper part of the rotating rod, the rotating guide wheel is movably connected with a rotating gear, a carrying disc is fixedly connected with the rotating gear, a reaction bottle is arranged above the carrying disc, heating is carried out to 190 ℃, reacting for 40min, filtering and removing the solvent, washing and drying by using distilled water and ethanol, thus obtaining the nickel-cobalt hydroxide nanosheet.
(2) Adding ethanol solvent, aluminum chloride and nickel cobalt hydroxide nanosheets into a reaction bottle, uniformly stirring, adding lithium hydroxide according to the mass ratio of 10:83:24, uniformly stirring for 2 hours, heating to 110 ℃, standing for 12 hours, placing a solid mixed product into a muffle furnace, heating to 500 ℃, carrying out heat treatment for 6 hours, then heating to 760 ℃, carrying out heat preservation and calcination for 8 hours, and preparing to obtain LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(3) Adding distilled water solvent and LiNi into a reaction bottle0.8Co0.15Al0.05O2Lamellar nanosheets, cobalt nitrate and nickel nitrate, ultrasubesUniformly dispersing by sound, adding urea with the mass ratio of 100:2.4:0.7:23, stirring for 1.5h, transferring the solution into a hydrothermal reaction kettle, heating to 130 ℃, reacting for 8h, filtering to remove the solvent, washing and drying by using distilled water and ethanol, placing the solid mixed product into a muffle furnace, heating to 450 ℃, and carrying out heat preservation treatment for 3h to prepare the porous NiCo2O4Coated LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(4) Adding porous NiCo to N-methylpyrrolidone solvent2O4Coated LiNi0.8Co0.15Al0.05O2Uniformly stirring the layered nanosheets, the conductive carbon black and the polyvinylidene fluoride in a mass ratio of 8:1:1 to form slurry, coating the slurry on the surface of an aluminum foil, drying, cutting by a sheet punching machine, and punching by a sheet pressing machine to obtain the porous NiCo2O4A lithium ion battery anode material 2 coated with nickel cobalt lithium aluminate.
Example 3
(1) Adding distilled water solvent, nickel chloride, cobalt chloride and urea with the mass ratio of 533:100:7600 into a reaction bottle, stirring and dissolving, adding ethylene glycol solvent, placing into a microwave reaction device, wherein the microwave reaction device comprises a microwave emitter, a motor is fixedly connected with the lower part of the interior of the microwave reaction device, the motor is movably connected with a rotating rod, a rotating guide wheel is fixedly connected with the upper part of the rotating rod, the rotating guide wheel is movably connected with a rotating gear, the rotating gear is fixedly connected with a carrying disc, the upper part of the carrying disc is provided with the reaction bottle, heating is carried out to 190 ℃, reacting for 30min, filtering and removing the solvent, washing and drying by using distilled water and ethanol, and preparing the nickel-cobalt hydroxide nanosheet.
(2) Adding ethanol solvent, aluminum chloride and nickel cobalt hydroxide nanosheets into a reaction bottle, uniformly stirring, adding lithium hydroxide according to the mass ratio of 10:84:25, uniformly stirring for 1.5h, heating to 110 ℃, standing for 12h, placing a solid mixed product into a muffle furnace, heating to 500 ℃, carrying out heat treatment for 5h, then heating to 740 ℃, carrying out heat preservation and calcination for 10h, and preparing to obtain LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(3) Adding distilled water solvent and LiNi into a reaction bottle0.8Co0.15Al0.05O2Adding urea after ultrasonic dispersion of the layered nanosheets, cobalt nitrate and nickel nitrate uniformly, stirring for 1.5h, transferring the solution into a hydrothermal reaction kettle, heating to 120 ℃, reacting for 6h, filtering to remove the solvent, washing and drying by using distilled water and ethanol, placing the solid mixed product in a muffle furnace, heating to 450 ℃, and carrying out heat preservation treatment for 2.5h to prepare the porous NiCo2O4Coated LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(4) Adding porous NiCo to N-methylpyrrolidone solvent2O4Coated LiNi0.8Co0.15Al0.05O2Uniformly stirring the layered nanosheets, the conductive carbon black and the polyvinylidene fluoride in a mass ratio of 8:1:1 to form slurry, coating the slurry on the surface of an aluminum foil, drying, cutting by a sheet punching machine, and punching by a sheet pressing machine to obtain the porous NiCo2O4A lithium ion battery anode material 3 coated with nickel cobalt lithium aluminate.
Example 4
(1) Adding distilled water solvent and nickel chloride, cobalt chloride and urea with the mass ratio of 535:100:7800 into a reaction bottle, stirring and dissolving, adding ethylene glycol solvent, placing in a microwave reaction device, wherein the microwave reaction device comprises a microwave emitter, a motor is fixedly connected below the inner part of the microwave reaction device, the motor is movably connected with a rotary rod, a rotary guide wheel is fixedly connected above the rotary rod, the rotary guide wheel is movably connected with a rotary gear, the rotary gear is fixedly connected with a carrying disc, the reaction bottle is arranged above the carrying disc, heating is carried out to 200 ℃, reacting for 40min, filtering and removing the solvent, washing and drying by using distilled water and ethanol, and preparing the nickel-cobalt hydroxide nanosheet.
(2) Adding ethanol solvent, aluminum chloride and nickel-cobalt hydroxide nanosheets into a reaction bottle, uniformly stirring, adding lithium hydroxide according to the mass ratio of 10:85:26, uniformly stirring for 2 hours, heating to 120 ℃, standing for 15 hours, placing a solid mixed product into a muffle furnace, heating to 520 ℃, carrying out heat treatment for 6 hours, and then heating to riseHeating to 760 ℃, and carrying out heat preservation calcination for 12h to prepare LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(3) Adding distilled water solvent and LiNi into a reaction bottle0.8Co0.15Al0.05O2Adding urea after ultrasonic dispersion of the layered nanosheets, cobalt nitrate and nickel nitrate uniformly, stirring for 2 hours, transferring the solution into a hydrothermal reaction kettle, heating to 130 ℃, reacting for 8 hours, filtering to remove the solvent, washing and drying by using distilled water and ethanol, placing the solid mixed product into a muffle furnace, heating to 480 ℃, and carrying out heat preservation treatment for 3 hours to prepare the porous NiCo2O4Coated LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(4) Adding porous NiCo to N-methylpyrrolidone solvent2O4Coated LiNi0.8Co0.15Al0.05O2Uniformly stirring the layered nanosheets, the conductive carbon black and the polyvinylidene fluoride in a mass ratio of 8:1:1 to form slurry, coating the slurry on the surface of an aluminum foil, drying, cutting by a sheet punching machine, and punching by a sheet pressing machine to obtain the porous NiCo2O4A lithium ion battery anode material 4 coated with nickel cobalt lithium aluminate.
Comparative example 1
(1) Adding distilled water solvent, namely nickel chloride, cobalt chloride and urea with the mass ratio of 528:100:7000 into a reaction bottle, stirring and dissolving, then adding ethylene glycol solvent, placing the mixture into a microwave reaction device, wherein the microwave reaction device comprises a microwave emitter, a motor is fixedly connected to the lower part of the interior of the microwave reaction device, the motor is movably connected with a rotating rod, a rotating guide wheel is fixedly connected to the upper part of the rotating rod, the rotating guide wheel is movably connected with a rotating gear, the rotating gear is fixedly connected with a carrying disc, the upper part of the carrying disc is provided with the reaction bottle, heating is carried out to 180 ℃, reacting for 40min, filtering and removing the solvent, washing and drying by using distilled water and ethanol, and preparing the nickel-cobalt hydroxide nanosheet.
(2) Adding ethanol solvent, aluminum chloride and nickel-cobalt hydroxide nanosheets into a reaction bottle, stirring uniformly, adding lithium hydroxide, and mixing the ethanol solvent, the aluminum chloride and the nickel-cobalt hydroxide nanosheetsStirring at a constant speed for 2h, heating to 120 ℃, standing for 10h, placing the solid mixed product in a muffle furnace, heating to 520 ℃, carrying out heat treatment for 4h, then heating to 760 ℃, and carrying out heat preservation and calcination for 8h to obtain the LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(3) Adding distilled water solvent and LiNi into a reaction bottle0.8Co0.15Al0.05O2Adding urea after ultrasonic dispersion of the layered nanosheets, cobalt nitrate and nickel nitrate uniformly, stirring for 2 hours, transferring the solution into a hydrothermal reaction kettle, heating to 110 ℃, reacting for 8 hours, filtering to remove the solvent, washing and drying by using distilled water and ethanol, placing the solid mixed product in a muffle furnace, heating to 420 ℃, and carrying out heat preservation treatment for 3 hours to prepare the porous NiCo2O4Coated LiNi0.8Co0.15Al0.05O2A layered nanosheet.
(4) Adding porous NiCo to N-methylpyrrolidone solvent2O4Coated LiNi0.8Co0.15Al0.05O2Uniformly stirring the layered nanosheets, the conductive carbon black and the polyvinylidene fluoride in a mass ratio of 8:1:1 to form slurry, coating the slurry on the surface of an aluminum foil, drying, cutting by a sheet punching machine, and punching by a sheet pressing machine to obtain the porous NiCo2O4Comparative example 1 shows a lithium ion battery positive electrode material coated with lithium nickel cobalt aluminate.
Porous NiCo in the examples and comparative examples, respectively2O4Lithium ion battery anode material coated with nickel cobalt lithium aluminate is used as a working anode, a lithium sheet is used as a working cathode, and 1mol/L LiPF6The solution of + ethylene carbonate + dimethyl carbonate + diethyl carbonate is used as electrolyte, Celgard2400 membrane is used as diaphragm, and assembled into CR2025 button cell in argon glove box, and electrochemical performance test is carried out in CT2001A blue battery test system, and the test standard is GB/T34131-.
Claims (1)
1. Porous NiCo2O4The preparation method of the anode material coated with the nickel-cobalt lithium aluminate is characterized by comprising the following steps: the method comprises the following steps:
(1) adding nickel chloride, cobalt chloride, urea and glycol solvent into a distilled water solvent, placing the mixture into a microwave reaction device, heating the mixture to 180 ℃ and 200 ℃, and reacting for 20-40min to prepare nickel-cobalt hydroxide nanosheets;
(2) adding aluminum chloride, nickel-cobalt hydroxide nanosheets and lithium hydroxide into an ethanol solvent, stirring at a constant speed for 1-2h, heating to 120 ℃ for 100-15 h, standing for 10-15h, placing a solid mixed product into a muffle furnace, heating to 520 ℃ for 480-6 h, performing heat treatment for 4-6h, then heating to 760 ℃ for 720-6 h, and performing heat preservation and calcination for 8-12h to obtain the LiNi0.8Co0.15Al0.05O2A layered nanosheet;
(3) adding LiNi into distilled water solvent0.8Co0.15Al0.05O2Adding urea after ultrasonic dispersion of the layered nano sheets, cobalt nitrate and nickel nitrate is uniform, stirring for 1-2h, transferring the solution into a hydrothermal reaction kettle, heating to 110-2O4Coated LiNi0.8Co0.15Al0.05O2A layered nanosheet;
(4) adding porous NiCo to N-methylpyrrolidone solvent2O4Coated LiNi0.8Co0.15Al0.05O2Uniformly stirring the layered nanosheets, the conductive carbon black and the polyvinylidene fluoride in a mass ratio of 8:1:1 to form slurry, coating the slurry on the surface of an aluminum foil, drying, cutting by a sheet punching machine, and punching by a sheet pressing machine to obtain the porous NiCo2O4A lithium ion battery anode material coated with nickel cobalt lithium aluminate;
the mass ratio of the nickel chloride, the cobalt chloride and the urea in the step (1) is 530-535:100: 7200-7800;
the microwave reaction device in the step (1) comprises a microwave emitter, a motor is fixedly connected to the lower portion of the inner portion of the microwave reaction device, the motor is movably connected with a rotating rod, a rotating guide wheel is fixedly connected to the upper portion of the rotating rod, the rotating guide wheel is movably connected with rotating wheel teeth, the rotating wheel teeth are fixedly connected with a carrying disc, and a reaction bottle is arranged above the carrying disc;
the mass ratio of the aluminum chloride to the nickel-cobalt hydroxide nanosheets to the lithium hydroxide in the step (2) is 10:82-85: 23-26;
LiNi in the step (3)0.8Co0.15Al0.05O2The mass ratio of the layered nanosheets to the cobalt nitrate to the nickel nitrate to the urea is 100:2-3.2:0.6-1: 20-30;
the porous NiCo2O4The nickel cobalt lithium aluminate-coated positive electrode material is prepared by microwave reaction by respectively using cobalt chloride and nickel chloride as a cobalt source and a nickel source, under the action of hydroxyl generated by urea hydrolysis, preparing a nano flaky nickel cobalt hydroxide precursor, and further reacting with aluminum chloride and lithium hydroxide to obtain LiNi with a two-dimensional layered appearance0.8Co0.15Al0.05O2A nanosheet structure;
the porous NiCo2O4In the high-temperature hydrothermal process of the nickel-cobalt lithium aluminate-coated positive electrode material, hydrolysis of urea releases hydroxyl and carbonate, the hydroxyl and the carbonate interact with cobalt ions and nickel ions to form a nano needle-shaped structure, the nano needle is self-assembled to form a nano sea urchin-shaped structure through an Oswald curing process to form a nano sea urchin-shaped double-metal carbonate hydroxide precursor, and further high-temperature heat treatment is carried out to generate NiCo2O4In the process, the precursor releases carbon dioxide and water vapor to form a hollow and mesoporous structure, thereby forming the sea urchin-shaped porous hollow NiCo2O4Coated LiNi0.8Co0.15Al0.05O2Lamellar nanosheets, NiCo2O4The coating effect is beneficial to reducing LiNi0.8Co0.15Al0.05O2The capacity of the anode material is attenuated, the rate capability of the anode material is improved, and simultaneously NiCo2O4Has good electricityThe unique sea urchin-shaped porous hollow structure can promote the migration of electrons, shorten the transmission path of lithium ions and accelerate the diffusion of the lithium ions, thereby reducing the polarization of the electrode and leading the porous NiCo2O4The positive electrode material coated with the nickel-cobalt lithium aluminate has excellent actual specific capacity and rate capability.
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